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इंटरनेट मानक Disclosure to Promote the Right To Information Whereas the Parliament of India has set

मानक

Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

जान1 का अ+धकार , जी1 का अ+धकार

Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

प0रा1 को छोड न' 5 तरफ

Jawaharlal Nehru

“Step Out From the Old to the New”

” Jawaharlal Nehru “Step Out From the Old to the New” IS 8602 (1977): Method of

IS 8602 (1977): Method of tests for chromate coatings on zinc and cadimium surfaces [MTD 24: Corrosion Protection]

on zinc and cadimium surfaces [MTD 24: Corrosion Protection] “ “ !ान $ एक न' भारत
“ “

!ान $ एक न' भारत का +नम-ण

ै”
ै”

Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह

Bhart hari—N īti ś atakam

“Knowledge is such a treasure which cannot be stolen”

 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 

IS:8602 - 1977

Indian Standard

METHODS

OF

TESTS

FOR

CHROMATE

CONVERSION COATINGS ON

ZINC

Metallic

AND

Finishes

CADMIUM

SURFACES

Sectional

Committee,

SMDC

23

Chairman

DR S. KRISRNAMURTRY

Indian

Telephone

Representing

Industries

Ltd,

Bangalore

Members

SHRI K. BALAKRISHANAN

Central

Electrochemical

Karaikudi

Research

Institute

Snnr S. R. NATARAJAN ( Alternate )

M. Y. BARKER SHRI P. K. SEN ( Alternate ) M. S, CHAKRA~ORT~

SHRI

Ministry

Premier

Canning

SRRI

SRRI AHINDRA CHATTERJEE

of

Defence

( DGI

)

Metal

Mitra

Finishers (P) Ltd, Calcutta

Phoenix

Ltd, Bombay

SHRI S. V. KULKARNI ( Alternate )

SHRI D. K. GaATTERJEE

CREMIST

8z

METALLURQIST,

Sen-Releigh

Ministry

of

Ltd,

Asansol

Railways

INTEGRAL

PERAMBUR CHEMIST& METALLURGIST11,

COACH

FAGTOW,

RESEARCH,

STANDARDSORGAKIZATION,

LUCKNOW ( Alternate )

DESIGNS AND

SHRI 0.

M. SINGHAL

SHRI KANTILAL T. DALAL SHRI JAYENDRA K.

SNRI P. K. DWSHPANDE

P. CHHABRA

Bharat Heavy

)

Kohinoor

Electric&

SHRI R.

( Alternate

Electra.Gilders,

Automobiles

DALAL ( Alternate ) The Premier

Ltd,

Ranipur

Bombay

Ltd,

Bombay

SHRI

A.

G.

PRARHU ( Alternate )

SHRI C. P. DEY SHRI M. Z. KHAN

SIJRI N. C. ROY ( Alternate

SHRIK.

A.

SIDDIQUI

1 )

( Alternate

Hindustan

Gcep Flashlight

Motors

Ltd,

Calcutta

Industries

Ltd, Allahabad

11 )

SRRI

U.

G. K. MENoN

Ministry

of

SHRI G. R. K. MURTHY ( A&z&

Snnr S. PANCHAPAKERAN

T.

)

I.

Cycles

SARI R. VENXATA~AMAN ( Alternate )

Defence

of India,

( R

&

D

Madras

)

( CSIR

( Continued

on page

2

@ Cop_vight

STANDARDS

under

the

1978

INSTITUTION

INDIAN

is protected

This

reproduction

publication

Zndian Copyright

Act

with written

( XIV

of

1957 )

of

in whole or in part

by any means except

permission

1 publisher

shall be deemed

to

be

an infringement

of copyright

under

the said

and

the

Act.

),

)

means except permission 1 publisher shall be deemed to be an infringement of copyright under the
IS:8602-1977 ( Continued from page 1 )   Members Representing   SHRI S. K. RAY

IS:8602-1977

( Continued from

page

1 )

 

Members

Representing

 

SHRI S. K. RAY

National

Metallurgical

Laboratory

( CSIR),

Jamshedpur

 

SRRI R.

SEN

Hindustan

Cables

Ltd,

Rupnarainpur

( District

Burdwan )

SHRI KALYAN SEIRI R. A. SHAH

GHO~H ( AEternute ) Ronuk

Industries Ltd,

Bombay

KUMARI

MRIDULA

A. SHAH

( Alternate

)

SRRI SURESH R. SHAH

Grauer and Weil ( India ) Ltd, Bombay

SHRI SUSRIL GOINKA ( Alfcrnate )

DR R. C. SHARMA

 

Eveready

Flashlight

Company,

Lucknow

SFIRIC. R. RAMA

RAO,

Director

General,

ISI

( Ex-o&o

Member

)

Director

( Strut

& Met

)

 

SHRI

S.

L.

BALI

Deputy

Director

( Met

),

IS1

Member ) Director ( Strut & Met )   SHRI S. L. BALI Deputy Director (
Member ) Director ( Strut & Met )   SHRI S. L. BALI Deputy Director (
Member ) Director ( Strut & Met )   SHRI S. L. BALI Deputy Director (

IS : 8602- 1977

Indian Standard

METHODS

OF

TESTS

FOR

CHROMATE

CONVERSION

COATINGS

ON

ZINC

AND

CADMIUM

SURFACES

COATINGS ON ZINC AND CADMIUM SURFACES 0. FOREWORD 0.1 This Indian Standard on 30 October 1977,

0.

FOREWORD

0.1 ThisIndian Standard

on 30 October 1977, after the draft finalized by the Metallic Finishes

was adopted

by the

Indian

Standards

Institution

Sectional Committee had been Division Council.

approved

by

the

Structural

and

Metals

0.2

The

methods

of

testing

chromate

 

conversion

coatings

relate

to

evaluation

of

the

protective

 

value

of

the

chemical

and

electrochemical

conversion

coatings

produced

by chromate

treatmentsof

zinc

and

cadmium

surfaces.

Passivation

has

little

effect

on

coating

thickness

of

zinc

and

cadmium.

 

The

protective

value

is

usually

determined

by

humidity

or

salt

spray

test.

Besides,

it

is

important

to

know

the

presence

of

the

colourless

chromate

coating

and

hexavalent

chromium

in both colourless

and

coloured

chromate

coatings.

The adhesion test has also been included

as

the

chromate

coatings

should

be

adherent

and

possess

adequate

abrasion

resistance.

0.3

In

reporting

the

result

of

a test

or analysis

made

in

accordance

with

this standard,

if

the

final

value,

observed

or calculated,

is to

be rounded

off:

it

shall

1. SCOPE

be

done

in

accordance

with

IS

: 2-1960”.

1.1

This

standard

covers

the methods

for

checking

the

required

characteristics

 

for

chemical

conversion

coatings

obtained

by

chromate

treatments

on

zinc

and

cadmium

surfaces.

 

2.

APPLICABILITY

 

2.1

The

methods

covered

in

this

standard

are

applicable

to

chromate

coatings

of

the

colourless

( both

one

and

two-dip

) iridescent

yellow

or

bronze,

olive

drab,

black,

colourless

anodic,

yellow

or black

anodic

types,

and

of

the

dyed

variety,

when

applied

to

surfaces

of

electro-‘deposited

zinc,

hot

dipped

zinc,

electro-deposlted

cadmium

and

zinc

die

castings.

*R&s

for rounding off numerical values ( revised ).

3

IS:860291977

2.2 In

carried

order

to

avoid

risk

the following

of

out within

uncertainties

time

limits:

in results,

these tests shall be

a) Minimum 24 hours after

the

application

of

the

chromate

conversion

coatings for all

tests

(

3

to 9

),

b) Maximum

3 days for tests

specified

in 3 and

4, and

 

c) 30 days for tests specified

Maximum

in

4,

6 and

7.

3.

TEST

COATING

FOR

PRESENCE

OF

A

COLOURLESS

CHROMATE

3.1 Test

[

PH of the solution

Solution

-

shall

Dissolve

1

in

50

g

of

lead

or deionized

acetate

trihydrate

The

Pb

( C2H302

)2.3H20

1 litre

of distilled

and 6.8.

water.

5.5

3.1.1 Any white precipitate formed during the initial preparation of

be between

the solution may be dissolved by small additions of -acetic acid, provided

that the pH is not reduced to a value below

white precipitate thereafter, the solution shall be discarded.

5’5. Upon formation of a

3.2 Procedure

3.2.1

Place

1 drop

of the test solution

on the surface

to be tested.

In

the case of a zinc substrate, observe the spot for 3 minutes. The presence of a colourless chromate conversion coating will be indicated when the formation of a dark or black stain is delayed by at least 1 minute after application of the test solution. Delay of black stain formation by more than 3 minutes may be indicative of supplementary coatings, such as wax or oil.

3.2.2 In the case of a cadmium substrate, observe the spot for 1 minute.

The presence of a colourless chromate conversion coating will be indicated when the formation of a dark or black stain is delayed by at least 6 seconds. Delay of black stain formation by more than 1 minute may be indicative of supplementary coatings, such as wax or oil.

a

chromate conversion coating will react with the lead acetate solution to

3.2.3 Zinc

and

cadmium

surfaces

which

have not been treated

with

form a black

stain

within

2 to 5 seconds.

3.2.4 No significance should be placed upon any differences in reaction

time to black spot formation between 1 and 3 minutes on a zinc substrate with colourless chromate conversion treatment, or between 6 and 60 seconds on a cadmium substrate with colourless chromate conversion treatment. Factors, such as substrate surface texture ( roughness ),

chromate film thickness variations ( due to processing conditions ), variations in the ambient temperature of the test, and precise pH control

of the lead acetate solution have an influence on the reaction

time,

I

and

4

IS:8602

-1977

therefore

stated.

chromate

preclude

Similarly,

treatment

any

rating

the

test

solutions.

may

based

not

be

upon

used

times

beyond

those

to compare

various

already

types

of

NOTE - Both colourless and coloured chromate conversion coatings which have lost their protective value through dehydration from exposure to temperatures in excess of 60°C will form black stain in less than 60 seconds on zinc, and less than

 

5 seconds

on

cadmium.

 

4.

TEST

FOR

PRESENCE

 

OF

HEXAVALENT

CHROMIUM

 

IN

BOTH

COLOURLESS

AND

COLOURED

CHROMATE

COATINGS

 

4.1

Test

Solution

-

Dissolve

0’4

g of diphenylcarbazide

in

a mixture

of

20

ml

of

acetone

and

20

ml

of ethanol.

After

dissolution,

add

20

ml

of

75 percent

phosphoric

acid

and

20

ml

of

distilled

water.

The

solution

shall

be

prepared

not

more

than

8 h prior

to

use.

4.2

Procedure

4.2.1

Place

1

to

5 drops

of the

test

solution

on

the

surface

to be

tested.

If hexavalent

chromium

is

present,

a red

to

violet

colour

will

appear

within

a few minutes.

Any

colour

which

appears

much

later,

for example,

on

drying,

may

be

disregarded.

 

4.2.2 For

comparative

purposes,

a

surface

that

is

known

not

to

have

been

chromate

treated

may

be similarly

tested.

5.

DETERMINATION

OF

HEXAVALENT

CHROMIUM

CONTENT

OF

BAZIDE

COLOURED

CHROMATE

( COLORIMETRIC

5.1 Reagents.

5.1.0 During

analysis,

use

only

COATINGS

)

METHOD

-

reagents

of recognized

DIPHENYLCAR-

analytical

grade,

and

only

distilled

water

or

water

of equivalent

purity.

5.1.1

Dilute

Sulphuric

Acid

-

1

:

3

( v/v

).

5.1.2 Diphcnylcarbazt’de

Solution

 

-

Dissolve

0.50

g of diphenylcarbazide

in

50

ml

of

acetone;

dilute

slowly,

while

stirring,

with

50

ml

of

water

( rapid

mixing

may

result

in

precipitation

of diphenylcarbazide

).

For

maximum stability,

keep

under

refrigeration

in

an

amber-coloured

glass

bottle.

 

5.1.3

Phosphate

Buffer

Solution

-

Dissolve

55

g

of

sodium

dihydrogen

orthophosphate

monohydrate

( NaHzPO,.HzO

)

in

100

ml

of water.

 
 

5.1.4

Standard

Potassium

Dichromate

Solution

-

Dilute

2

ml

of

standard

potassium dichromate

solution

( 0.1

N

)

to

1 litre.

One

millilitre

of this

solution contains 3*47/pg of chromium.

 

A solution

containing

9.90

mg/l

of

potassium

dichromate

contains

3.5

5

pg/ml

of

chromium.

IS : 8602 - 1977 5.2 Apparatus 5.2.1 Ordinary having be set for length of

IS

: 8602

- 1977

5.2 Apparatus

5.2.1 Ordinary

having

be

set for

length

of

laboratory

may

be

apparatus

used.

With

of

An

in either

and

photoelectric

photoelectric

absorption

case.

calorimeter

calorimeter,

of

an

or

use

540 nm

spectrophotometer

a filter

shall

path

a

520 nm.

a mean

transmission

A wavelength

cell

with

a spectrophotometer.

1 cm

shall

be used

optical

5.3 procedure

for

Calibration

5.3.1

Preparation of Calibration Curve -

To

a series

of

five

250-ml

volu-

metric

flasks,

add

respectively

0,

10,

20,

30

and

40

ml

of

the

standard

potassium

dichromate

solulion.

 

Add

to each

100 ml

of

water

and

3

ml

of

dilute

sulphuric

acid.

Take

each

flask

through

the

following

steps,

one

flask

at

a time,

add

3 ml

of

the

diphenylcarbazide

solution

and

mix

well.

solution,

Exactly

dilute

2 minutes

to the

after

mark

5.3.2

read

in

Transfer

a

portion

the

calorimeter

or

mixing,

mix.

and

add

25

solution

spectrophotometer.

of

each

ml

to

of

the

phosphate

buffer

an

absorption

Each

reading

cell

shall

and

be

completed

within

25

minutes

 

after

addition

of

the

diphenylcarbazide

 

solution

because

the

colour

is

not

stable.

Subtract

the

blank

(

0

ml

)

from

each

reading

 

and

plot

the

differences

 

against

micrograms

of

chromium

per

250

ml.

5.4

Blank

Test

-

Carry

out

a blank

test

on

the

reagents

simultaneously

 

with

the

determination.

 

5.5

Procedure

 

for

Testing--P

repare

a test

piece

measuring

mately 50 X 100 mm.

Heat

50

ml

of distilled

water

to boiling

approxi- in a 400_~1

beaker, then introduce

the

test

piece.

Leach

for

exactly

5 minutes

while

the

water

continues

to boil,

remove

the

test

piece,

rinse

into the beaker,

cool

the

beaker

and

contents

to

room

temperature,

add

3 ml

of

dilute

sulphuric

acid,

mix,

transfer

to

a

lOO-mi

vohrmetric

flask,

add

3 ml

of

diphenylcarbazide

 

solution

and

mix

well.

Exactly

2

minutes

after

mixing,

add

25

ml

of

phosphate

buffer

solution,

dilute

to the

mark

and

mix.

Two

minutes

after

the

addition

of

the

diphenylcarbazide

solution,

 

transfer

a

portion

of

the

solution

to

an

absorption

cell

and

read

in

the

calorimeter

or

spectrophotometer.

appropriate

calibration

curve,

into

Convert

micrograms

the

per

reading,

ml.

100

using

the

5.6

Calculation

-

Deduct

the

reading

obtained

for the blank

and deter-

mine

the

hexavalent

chromium

content

of

the

film

by

reference

to the

calibration

curve

or

by the

use of

a factor

derived

from

it.

hexavalent

chromium

content

*by

the

surface

area

of

the

obtain

the

hexavalent

chrommm

content

in

milligrams

Divide

test

piece

the

to

per

square

centimetre.

the hexavalent chrommm content in milligrams D i v i d e test piece t h
 

IS : 8602-

1977

6.

DETERMINATION

OF

TOTAL

 

CHROMIUM

CONTENT

OF

COLOURED

CHROMATE

COATINGS-DIPHENYLCARBAZIDE

( COLORIMETRIC

) METHOD

 

6.1 Reagents

 

6.1.0 During

the

analysis,

use

only

reagents

of

recognized

analytical

grade,

and

only

distilled

water

or

water

of

equivalent

purity.

 

6.1.1

Standard

Potaesium Dichromate

 

Solution -

see 5.1.4.

 

6.1.2

Dilute

Sulphuric

Acid -

1

: 3

( v/v ).

 

6.1.3

Phosphate Bugler Solution -

see 5.1.3.

 

6.1.4

Di’henylcarbazide

Solution -

see 5.1.2.

6.1.5

Ammonium

Persulphate

[

( NH4

)2&Os]

-

solid.

 

6.1.6

Silver

Nitrate

Solution -

( 0’1

 

N

)

17 g/l.

 

6.1.7

Sodium Hydroxide

Solution -

 

(

6

N

)

240

g/l.

6.2

Apparatus

-

see 5.2.

 

6.3

Procedure

for

Calibration

 

6.3.1

Preparation

of

Calibration

Curve -

 

To

a

series

of

five

250-m]

volumetric

flasks,

add

respectively

0,

10,

20,

30

and

40 ml

of the

standard

potassium

dichromate

solution.

Add

to each

100

ml

of

water

and

3 ml

of

dilute

sulphuric

acid.

Take

each

 

flask

through

the

following

steps,

one

flask

at

a time;

add

3 ml

of the

diphenylcarbazide

solution

and

mix

well.

Exactly

2 minutes

after

mixin,, m add

25

ml

of the

phosphate

buffer

solution,

dilute

to

the

mark

and

mix.

6.3.2

Transfer

a portion

of each

solution

to an absorption

cell and read

in

the colorimeter’or spectrophotometer.

Each

reading

shall

be completed

within 25 minutes after addition of the diphenylcarbazide

solution because

 

Subtract

the

blank

(

0

ml

)

from

each

reading

the colour is not stable. and plot the differences

against

micrograms

of

chromium

per 250 ml.

 

6.3.3

Blank

Test

-

Carry

out

a

blank

test

on

the

reagents

simulta-

neously

with

the

determination.

 

6.4

Procedure

for

 

Testing-

Prepare

a test

piece

 

measuring

approxi-

mately

50

x

100

mm.

Heat

25

ml

of

dilute

sulphuric

acid

to 40

to 50°C

and

pour

into

a beaker

containing

the

test

piece.

Swirl

continuously

 

so

that

all

surfaces

are

exposed

to acid

for

10

to

15

seconds.

Remove

the

test

piece,

and

rinse

into

the

beaker.

Dilute

to

about

175

ml,

and

add

about

0.1

g

of

the

ammonium

persulphate

and

3 ml

 

of

the

silver

nitrate

solution.

Then

add

boiling

chips

and

boil

for

30

minutes.

Cool,

and

adjust

the PH

to

1’5

to

1.8

with

the

sodium

 

hydroxide

solution

( about

20 ml;

to measure

the

pH,

transfer

a drop

to PH

paper-do

 

not

immerse

the

paper

in

the

solution

).

Transfer

to a 250-ml

volumetric

flask.

Rinse

the

beaker

twice

into

the

flask

with

10

to

15

ml

of

water,

add

3

ml

I

of

7

1s t 8602 - 1977   diphenylcarbazide   solution, and mix. E x a c

1s t 8602

- 1977

 

diphenylcarbazide

 

solution,

and

mix.

Exactly

2 minutes

after

addition

of the

diphenylcarbazide

solution,

add

25

ml of phosphate

buffer solution,

dilute

to the

mark

and

mix.

Transfer

a

portion

of

the

solution

to

an

absorption

cell

and

read

in

the

calorimeter

or

spectrophotometer.

Convert the reading, micrograms per 250 ml.

using

the

appropriate

calibration

curve,

into

6.5

Calculation

-

Deduct

the

reading

obtained

for

the

blank

and

determine

the

total

chromium

content

of

the

film

by

reference

to

the

calibration

curve

or by

use

of

a factor

derived

from

it.

Divide

the

total

chromium

content

by

the

surface

area

of

the

test

piece

to obtain

the

total

chromium

content

in

milligrams

per

square

centimetre.

7. DETERMINATION

OF COATING

MASS

PER

UNIT

AREA

OF

BOTH

COATINGS

COLOURLESS

AND

7.1 This

testing

shall

be

conversion

done

in

coating

accordance

mass

per

COLOURED

CHROMATE

with

unit

Indian

area

by

Standard

methods

of

gravimetric

method

(under

preparation

) ‘.

NOTE-

Until

this standard

is published,

the method

of

testing conversion

coatings

shall be as agreed

to between

the purchaser

and

the supplier.

 

8.

ADHESION

TEST

8.1

Test

adhesion

of a coloured

chromate

coating

by

rubbing

the surface

with

a soft

white

tissue

paper

or

with

a gritless

gum

eraser,

using

normal

hand

pressure

( about

10 strokes

).

There

shall

be

no

appreciable

stain-

ing

on

the

tissue

paper

when

this

is

used

for

the

test,

nor

shall

the

chromate

coating

be removed

or

worn

through

to

the

underlying

zinc

or

cadmium

when

rubbed

with

the

paper

or

the

eraser.

 

9.

HUMIDITY

OR

SALT

SPRAY

TEST

9.1

Humidity

Test

9.1.1 Apparatus

-

A heat

insulated

chamber:

a) A fan to circulate

the

air

in

the

chamber,

b) and

A non-metallic

non-corrosive

support

for

the

specimen

near

the centre

of

the

chamber.

 

9.1.2 Temperature

ature

of

55

f

2”C,

of

Test

-

followed

The

test

by

cooling

shall

be

to 30°C.

conducted

at

a

temper-

 

9.1.3

Humidip

-

The

relative

humidity

shall

not

be

less

than

95

percent.

 

9.1.4

Test

Cycle

-

The

coating

shall

be

subjected

to

the

above-

mentioned